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4-Fluorobenzyl bromide → 2-(5-(4-Fluoro-benzyl)-furan-2-yl)-[1,3]dioxolane

HRID 640527
ノート
印刷プレビュー

反応式

HRID 640527 の反応式
[O:1]1[CH2:5][CH2:4][O:3][CH:2]1[C:6]1[O:7][CH:8]=[CH:9][CH:10]=1.C([Li])CCC.[F:16][C:17]1[CH:24]=[CH:23][C:20]([CH2:21]Br)=[CH:19][CH:18]=1>O1CCCC1>[F:16][C:17]1[CH:24]=[CH:23][C:20]([CH2:21][C:8]2[O:7][C:6]([CH:2]3[O:3][CH2:4][CH2:5][O:1]3)=[CH:10][CH:9]=2)=[CH:19][CH:18]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 680214-Fluorobenzyl bromideHCID 2631582-Furyl-1,3-dioxolaneHCID 178418339Butyllithium

生成物 1

HCID 592550712-(5-(4-Fluoro-benzyl)-furan-2-yl)-[1,3]dioxolane収率 51%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a tetrahydrofuran (50 mL) solution of 2-(1,3-dioxolan-2-yl-furan (5 g, 35.7 mmol) was added n-butyl lithium (15.6 mL, 2.64 M hexane solution, 41.1 mmol) at −78° C., which was stirred for 1 hour at that temperature. A tetrahydrofuran solution of 4-fluorobenzyl bromide (6.9 g, 36.5 mmol) was added dropwise to this mixture, which was stirred for another hour at −78° C. The mixture was raised to room temperature and partitioned into ethyl acetate and a saturated ammonium chloride aqueous solution. The organic layer was separated, washed with saturated aqueous sodium chloride, dried over anhydrous magnesium sulfate, and filtered. The filtrate was concentrated under a reduced pressure, and the residue was purified by silica gel column chromatography (ethyl acetate:heptane=1:10 to 1:3) to obtain the title compound (4.51 g, 51%).

後処理

  1. stirringwas stirred for another hour at −78° C
  2. custompartitioned into ethyl acetate
  3. customThe organic layer was separated
  4. washwashed with saturated aqueous sodium chloride
  5. dry with materialdried over anhydrous magnesium sulfate
  6. filtrationfiltered
  7. concentrationThe filtrate was concentrated under a reduced pressure
  8. customthe residue was purified by silica gel column chromatography (ethyl acetate:heptane=1:10 to 1:3)

出典と根拠

ORDレコード
ord-aeed3e180a8144aea77f276ed28aaf5c
出典データセット
uspto-grants-2010_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07691882B2

反応ノート

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